CN102030310A - Method for preparing Si/Mn27Si47 core-shell structure nanowire array - Google Patents

Method for preparing Si/Mn27Si47 core-shell structure nanowire array Download PDF

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CN102030310A
CN102030310A CN 201010538262 CN201010538262A CN102030310A CN 102030310 A CN102030310 A CN 102030310A CN 201010538262 CN201010538262 CN 201010538262 CN 201010538262 A CN201010538262 A CN 201010538262A CN 102030310 A CN102030310 A CN 102030310A
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shell structure
silicon substrate
monocrystalline silicon
nanowire array
tube furnace
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CN102030310B (en
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师文生
刘海龙
佘广为
凌世婷
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Technical Institute of Physics and Chemistry of CAS
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Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a method for preparing a Si/Mn27Si47 core-shell structure nanowire array. The method comprises the following steps of: soaking a monocrystalline silicon substrate of which the surface is etched with a silicon nanowire array which is vertically and directionally arranged in ethanol solution of MnCl2; taking out and naturally air-drying; placing the air-dried monocrystalline silicon substrate into an alumina porcelain boat; placing the boat in the center of a tubular furnace; introducing inert gas serving as protective gas into the tubular furnace, wherein the pressure intensity in the tubular furnace is 70Pa; heating the tubular furnace to 750 DEG C; and preserving heat at the temperature of 750 DEG C for 300 minutes to obtain the Si/Mn27Si47 core-shell structure nanowire array on the monocrystalline silicon substrate. The method for preparing the Si/Mn27Si47 core-shell structure nanowire array is simple and practicable; and the prepared Si/Mn27Si47 core-shell structure nanowire array has great potential application value in Si nanowire-based infrared detectors, solar photovoltaic devices and electron spin devices.

Description

Si/Mn 27Si 47The preparation method of nuclear shell structure nano linear array
Technical field
The invention belongs to the preparing technical field of conductor nano tube/linear array, particularly a kind of Si/Mn 27Si 47The preparation method of nuclear shell structure nano linear array.
Background technology
Monodimension nanometer material presents a lot of peculiar character with respect to traditional material, is demonstrating important effect aspect Jie's sight field and the nano-device development.For example, they can be used as line in the needle point of PSTM, various sensor, microelectrode and the super large integrated circuit, optical fiber, microbit etc.Mn 27Si 47Being a kind of transition metal silicide, specifically is again a kind of in the high manganese silicon compound in the manganese silicon compound series.Mn 27Si 47As a kind of transition metal silicide, possess a series of excellent properties of transition metal silicide, low as anti-oxidant, resistance to chemical attack, heat endurance height, resistivity, with the fabulous compatibility of Si device, form Ohmic contact etc. easily with the Si material.While Mn 27Si 47A kind of as in the high manganese silicon compound possesses the characteristic of high manganese silicon compound again, as narrow energy gap, good thermoelectricity capability, good ferromagnetic property.When the size of material reaches the yardstick of nanometer scale, show some new physics and electronics properties possibly, as high manganese silicon compound Mn 19Si 33The thermoelectricity capability of nano wire has obtained enhancing because of the reason of surphon scattering, and high manganese silicon compound Mn 4Si 7The ferromagnetic property of nano wire also is enhanced because of the dimensional effect of nanostructured.Same Mn as high manganese silicon compound 27Si 47, its monodimension nanometer material also possesses new physics and electronics property probably, thereby has huge potential using value aspect Infrared Detectors, solar photovoltaic device, the electron spin device.Up to the present, also do not find relevant preparation Mn 27Si 47The report of monodimension nanometer material, and the present invention adopts a kind of new simple method to prepare Si/Mn just 27Si 47The nuclear shell structure nano linear array.
Summary of the invention
The purpose of this invention is to provide a kind of Si/Mn 27Si 47The preparation method of nuclear shell structure nano linear array.
Si/Mn of the present invention 27Si 47The preparation method of nuclear shell structure nano linear array may further comprise the steps:
1) adopt the method for chemical etching to prepare silicon nanowire array: will place the mixed solution of silver nitrate and hydrofluoric acid to soak 3 minutes with the monocrystalline silicon substrate that hydrofluoric acid clean is crossed; Wherein, the concentration of the silver nitrate in the mixed solution of silver nitrate and hydrofluoric acid is 5mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; The monocrystalline silicon substrate immersion pernitric acid is silver-colored and the hydrofluoric acid mixed solution takes out in the etching solution that is placed on hydrogen peroxide and hydrofluoric acid mixing and carries out etching, wherein, the concentration of the hydrogen peroxide in the etching solution that hydrogen peroxide and hydrofluoric acid mix is 4mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; Etching temperature is 50 ℃, and etch period is 15 minutes, at the monocrystalline silicon substrate surface deposition silver ion place is arranged, Si can be etched down, and not depositing the silver ion place, Si can be retained, thereby goes out the silicon nanowire array that vertical orientation is stood and arranged in the monocrystalline silicon substrate surface etch;
2) surface etch that step 1) is obtained goes out the stand monocrystalline silicon substrate of the silicon nanowire array arranged of vertical orientation and places MnCl 2Ethanolic solution in soak (preferred soak time is 10 minutes), take out the back and dry naturally;
3) with step 2) monocrystalline silicon substrate that dries puts into the aluminium oxide porcelain boat, the aluminium oxide porcelain boat put into the center of tube furnace again; Feed inert gas (as Ar gas) as protective gas (flow of preferred inert gas (as Ar gas) is 100sccm) in tube furnace, the pressure in the tube furnace is 70Pa; It is 750 ℃ that tube furnace is heated to temperature, is 750 ℃ in temperature and is incubated 300 minutes down, obtains Si/Mn on monocrystalline silicon substrate 27Si 47The nuclear shell structure nano linear array.
Described MnCl 2The concentration of ethanolic solution be preferably 0.1～1mol/L.
Described Si/Mn 27Si 47The Mn of nuclear shell structure nano linear array 27Si 47Shell is a mono-crystalline structures, and the diameter of nano wire is 100～300nm, and length is 10 μ m.
The present invention is that the silicon nanowire array prepared with chemical etching method is as the silicon source, with MnCl 2For the Mn source, obtain Si/Mn by reaction in-situ 27Si 47The nuclear shell structure nano linear array, preparation method of the present invention is simple, and the Si substrate that has the Si nano-wire array is positioned over MnCl 2Ethanolic solution in soak, on the Si nano-wire array, superscribed one deck MnCl 2Film, insulation (annealing) 300 minutes under 750 ℃ temperature then makes MnCl 2Obtained Si/Mn with the reaction of Si nano-thread in-situ 27Si 47The nuclear shell structure nano linear array.The present invention can be by control MnCl 2The concentration of ethanolic solution, change Mn 27Si 47The thickness of shell, MnCl 2The concentration of solution is dense more, Mn 27Si 47Shell thickness thick more, the Si/Mn that obtains 27Si 47Mn in the nuclear shell structure nano linear array 27Si 47Be mono-crystalline structures, the diameter of nano wire is 100～300nm, and length is 10 μ m.
The Si/Mn that the present invention is prepared 27Si 47The nuclear shell structure nano linear array has huge potential using value aspect the Infrared Detectors of Si nano wire, solar photovoltaic device, electron spin device.
Description of drawings
Fig. 1. the positive SEM picture of the silicon nanowire array that obtains with the method for chemical etching.
Fig. 2. the side SEM picture of the silicon nanowire array that obtains with the method for chemical etching.
Fig. 3. the single Si/Mn of the embodiment of the invention 1 27Si 47The TEM picture of nuclear shell structure nano line.
Fig. 4. the Si/Mn of the embodiment of the invention 3 27Si 47The SEM picture of nuclear shell structure nano linear array.
Fig. 5. the single Si/Mn of the embodiment of the invention 3 27Si 47The TEM picture of nuclear shell structure nano line.
Fig. 6. the Si/Mn of the embodiment of the invention 3 27Si 47The XRD spectra of nuclear shell structure nano linear array.
Fig. 7. the single Si/Mn of the embodiment of the invention 4 27Si 47The TEM picture of nuclear shell structure nano line.
The specific embodiment
Embodiment 1
1) will place the mixed solution of silver nitrate and hydrofluoric acid to soak with the monocrystalline silicon substrate that hydrofluoric acid clean is crossed 3 minutes; Wherein, the concentration of the silver nitrate in the mixed solution of silver nitrate and hydrofluoric acid is 5mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; The monocrystalline silicon substrate immersion pernitric acid is silver-colored and the hydrofluoric acid mixed solution takes out in the etching solution that is placed on hydrogen peroxide and hydrofluoric acid mixing and carries out etching, wherein, the concentration of the hydrogen peroxide in the etching solution that hydrogen peroxide and hydrofluoric acid mix is 4mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; In water-bath, carry out etching, bath temperature is 50 ℃, etch period is 15 minutes, at the monocrystalline silicon substrate surface deposition silver ion place is arranged, Si can be etched down, and not depositing the silver ion place, Si can be retained, thereby goes out the silicon nanowire array that vertical orientation is stood and arranged in the monocrystalline silicon substrate surface etch; Wherein, the diameter of silicon nanowires is 100～300nm, about the about 10 μ m of length; The SEM pattern of the silicon nanowire array that obtains as depicted in figs. 1 and 2.
2) surface etch that step 1) is obtained goes out vertical orientation and stands that to place concentration be the MnCl of 0.1mol/L for the monocrystalline silicon substrate of the silicon nanowire array arranged 2Ethanolic solution in soaked 10 minutes, take out the back and dry naturally; To dry the back monocrystalline silicon substrate then and put into the aluminium oxide porcelain boat, again the aluminium oxide porcelain boat be put into the center of tube furnace; With tube furnace be heated to temperature be 750 ℃ after the insulation 300 minutes; In whole heating and insulating process, in tube furnace, feed Ar gas as protective gas, the flow of Ar gas is 100sccm, the pressure in the tube furnace is 70Pa; After treating that furnace temperature drops to room temperature, take out sample, on monocrystalline silicon substrate, obtained Si/Mn 27Si 47The nuclear shell structure nano linear array, the Si/Mn that obtains 27Si 47The length of the nano wire in the nuclear shell structure nano linear array is about 10 μ m, and diameter is 100～300nm, the TEM pattern of single nano-wire as shown in Figure 3, Mn as can be seen 27Si 47Shell is a mono-crystalline structures, and shell thickness is about 2nm.
Embodiment 2
1) will place the mixed solution of silver nitrate and hydrofluoric acid to soak with the monocrystalline silicon substrate that hydrofluoric acid clean is crossed 3 minutes; Wherein, the concentration of the silver nitrate in the mixed solution of silver nitrate and hydrofluoric acid is 5mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; The monocrystalline silicon substrate immersion pernitric acid is silver-colored and the hydrofluoric acid mixed solution takes out in the etching solution that is placed on hydrogen peroxide and hydrofluoric acid mixing and carries out etching, wherein, the concentration of the hydrogen peroxide in the etching solution that hydrogen peroxide and hydrofluoric acid mix is 4mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; In water-bath, carry out etching, bath temperature is 50 ℃, etch period is 15 minutes, at the monocrystalline silicon substrate surface deposition silver ion place is arranged, Si can be etched down, and not depositing the silver ion place, Si can be retained, thereby goes out the silicon nanowire array that vertical orientation is stood and arranged in the monocrystalline silicon substrate surface etch; Wherein, the diameter of silicon nanowires is 100～300nm, about the about 10 μ m of length.
2) surface etch that step 1) is obtained goes out vertical orientation and stands that to place concentration be the MnCl of 0.3mol/L for the monocrystalline silicon substrate of the silicon nanowire array arranged 2Ethanolic solution in soaked 10 minutes, take out the back and dry naturally; To dry the back monocrystalline silicon substrate then and put into the aluminium oxide porcelain boat, again the aluminium oxide porcelain boat be put into the center of tube furnace; With tube furnace be heated to temperature be 750 ℃ after the insulation 300 minutes; In whole heating and insulating process, in tube furnace, feed Ar gas as protective gas, the flow of Ar gas is 100sccm, the pressure in the tube furnace is 70Pa; After treating that furnace temperature drops to room temperature, take out sample, on monocrystalline silicon substrate, obtained Si/Mn 27Si 47The nuclear shell structure nano linear array, the Si/Mn that obtains 27Si 47The length of the nano wire in the nuclear shell structure nano linear array is about 10 μ m, and diameter is 100～300nm, Mn 27Si 47Shell is a mono-crystalline structures.
Embodiment 3
1) will place the mixed solution of silver nitrate and hydrofluoric acid to soak with the monocrystalline silicon substrate that hydrofluoric acid clean is crossed 3 minutes; Wherein, the concentration of the silver nitrate in the mixed solution of silver nitrate and hydrofluoric acid is 5mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; The monocrystalline silicon substrate immersion pernitric acid is silver-colored and the hydrofluoric acid mixed solution takes out in the etching solution that is placed on hydrogen peroxide and hydrofluoric acid mixing and carries out etching, wherein, the concentration of the hydrogen peroxide in the etching solution that hydrogen peroxide and hydrofluoric acid mix is 4mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; In water-bath, carry out etching, bath temperature is 50 ℃, etch period is 15 minutes, at the monocrystalline silicon substrate surface deposition silver ion place is arranged, Si can be etched down, and not depositing the silver ion place, Si can be retained, thereby goes out the silicon nanowire array that vertical orientation is stood and arranged in the monocrystalline silicon substrate surface etch; Wherein, the diameter of silicon nanowires is 100～300nm, about the about 10 μ m of length.
2) surface etch that step 1) is obtained goes out vertical orientation and stands that to place concentration be the MnCl of 0.5mol/L for the monocrystalline silicon substrate of the silicon nanowire array arranged 2Ethanolic solution in soaked 10 minutes, take out the back and dry naturally; To dry the back monocrystalline silicon substrate then and put into the aluminium oxide porcelain boat, again the aluminium oxide porcelain boat be put into the center of tube furnace; With tube furnace be heated to temperature be 750 ℃ after the insulation 300 minutes; In whole heating and insulating process, in tube furnace, feed Ar gas as protective gas, the flow of Ar gas is 100sccm, the pressure in the tube furnace is 70Pa; After treating that furnace temperature drops to room temperature, take out sample, on monocrystalline silicon substrate, obtained Si/Mn 27Si 47The nuclear shell structure nano linear array, the Si/Mn that obtains 27Si 47The length of the nano wire in the nuclear shell structure nano linear array is about 10 μ m, and diameter is 100～300nm, the SEM shape appearance figure as shown in Figure 4, the TEM pattern of single nano-wire as shown in Figure 5, Mn as can be seen 27Si 47Shell is a mono-crystalline structures, and shell thickness is about 25nm, its XRD spectra as shown in Figure 6, except that the diffraction maximum from Si substrate and Si nuclear structure, remaining diffraction maximum is all from Mn 27Si 47
Embodiment 4
1) will place the mixed solution of silver nitrate and hydrofluoric acid to soak with the monocrystalline silicon substrate that hydrofluoric acid clean is crossed 3 minutes; Wherein, the concentration of the silver nitrate in the mixed solution of silver nitrate and hydrofluoric acid is 5mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; The monocrystalline silicon substrate immersion pernitric acid is silver-colored and the hydrofluoric acid mixed solution takes out in the etching solution that is placed on hydrogen peroxide and hydrofluoric acid mixing and carries out etching, wherein, the concentration of the hydrogen peroxide in the etching solution that hydrogen peroxide and hydrofluoric acid mix is 4mmol/L, and the concentration of hydrofluoric acid is 4.8mol/L; In water-bath, carry out etching, bath temperature is 50 ℃, etch period is 15 minutes, at the monocrystalline silicon substrate surface deposition silver ion place is arranged, Si can be etched down, and not depositing the silver ion place, Si can be retained, thereby goes out the silicon nanowire array that vertical orientation is stood and arranged in the monocrystalline silicon substrate surface etch; Wherein, the diameter of silicon nanowires is 100～300nm, about the about 10 μ m of length.
2) surface etch that step 1) is obtained goes out vertical orientation and stands that to place concentration be the MnCl of 1.0mol/L for the monocrystalline silicon substrate of the silicon nanowire array arranged 2Ethanolic solution in soaked 10 minutes, take out the back and dry naturally; To dry the back monocrystalline silicon substrate then and put into the aluminium oxide porcelain boat, again the aluminium oxide porcelain boat be put into the center of tube furnace; With tube furnace be heated to temperature be 750 ℃ after the insulation 300 minutes; In whole heating and insulating process, in tube furnace, feed Ar gas as protective gas, the flow of Ar gas is 100sccm, the pressure in the tube furnace is 70Pa; After treating that furnace temperature drops to room temperature, take out sample, on monocrystalline silicon substrate, obtained Si/Mn 27Si 47The nuclear shell structure nano linear array, the Si/Mn that obtains 27Si 47The length of the nano wire in the nuclear shell structure nano linear array is about 10 μ m, and diameter is 100～300nm, the TEM pattern of single nano-wire as shown in Figure 7, Mn as can be seen 27Si 47Shell is a mono-crystalline structures, and shell thickness is about 50nm.

Claims (5)

1. Si/Mn 27Si 47The preparation method of nuclear shell structure nano linear array is characterized in that, this method may further comprise the steps:
1) adopt the method for chemical etching to go out the silicon nanowire array that vertical orientation is stood and arranged in the monocrystalline silicon substrate surface etch;
2) surface etch that step 1) is obtained goes out the stand monocrystalline silicon substrate of the silicon nanowire array arranged of vertical orientation and places MnCl 2Ethanolic solution in soak, dry after the taking-up;
3) with step 2) monocrystalline silicon substrate that dries puts into the aluminium oxide porcelain boat, the aluminium oxide porcelain boat put into the center of tube furnace again; Feed inert gas as protective gas in tube furnace, the pressure in the tube furnace is 70Pa; It is 750 ℃ that tube furnace is heated to temperature, is 750 ℃ in temperature and is incubated 300 minutes down, obtains Si/Mn on monocrystalline silicon substrate 27Si 47The nuclear shell structure nano linear array.
2. method according to claim 1 is characterized in that: step 2) described in MnCl 2The concentration of ethanolic solution be 0.1～1mol/L.
3. want 1 described method according to right, it is characterized in that: step 2) described in time of immersion be 10 minutes.
4. method according to claim 1 is characterized in that: the flow of the described inert gas of step 3) is 100sccm.
5. method according to claim 1 is characterized in that: described Si/Mn 27Si 47The Mn of nuclear shell structure nano linear array 27Si 47Shell is a mono-crystalline structures, and the diameter of nano wire is 100～300nm, and length is 10 μ m.
CN2010105382625A 2010-11-10 2010-11-10 Method for preparing Si/Mn27Si47 core-shell structure nanowire array Expired - Fee Related CN102030310B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103159501A (en) * 2012-11-15 2013-06-19 中国科学院理化技术研究所 Preparation method of core shell Si/Fe2O3 nanowire array
CN105841823A (en) * 2016-04-14 2016-08-10 董友强 Manganese-silicon nanowire infrared detector and manufacturing method thereof

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WO2008025962A1 (en) * 2006-08-31 2008-03-06 Cambridge Enterprise Limited Nanomaterial polymer compositions and uses thereof
CN101613881A (en) * 2009-07-22 2009-12-30 中国科学院理化技术研究所 A kind of method for preparing the SiC nano-wire array

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
WO2008025962A1 (en) * 2006-08-31 2008-03-06 Cambridge Enterprise Limited Nanomaterial polymer compositions and uses thereof
CN101613881A (en) * 2009-07-22 2009-12-30 中国科学院理化技术研究所 A kind of method for preparing the SiC nano-wire array

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《材料科学与工艺》 20080630 张慧云等 锰硅化合物的制备及塞贝克效应 第427-429页 1-5 第16卷, 第3期 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103159501A (en) * 2012-11-15 2013-06-19 中国科学院理化技术研究所 Preparation method of core shell Si/Fe2O3 nanowire array
CN103159501B (en) * 2012-11-15 2014-08-20 中国科学院理化技术研究所 Preparation method of core shell Si/Fe2O3 nanowire array
CN105841823A (en) * 2016-04-14 2016-08-10 董友强 Manganese-silicon nanowire infrared detector and manufacturing method thereof

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